CN109180142A - Aerosil composite insulation material and preparation method thereof - Google Patents
Aerosil composite insulation material and preparation method thereof Download PDFInfo
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- CN109180142A CN109180142A CN201811222567.8A CN201811222567A CN109180142A CN 109180142 A CN109180142 A CN 109180142A CN 201811222567 A CN201811222567 A CN 201811222567A CN 109180142 A CN109180142 A CN 109180142A
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- composite insulation
- insulation material
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- fiber
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 135
- 239000002131 composite material Substances 0.000 title claims abstract description 49
- 239000012774 insulation material Substances 0.000 title claims abstract description 45
- 229910002012 Aerosil® Inorganic materials 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 42
- 239000000835 fiber Substances 0.000 claims abstract description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 23
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 21
- 229960001866 silicon dioxide Drugs 0.000 claims abstract description 21
- 235000019441 ethanol Nutrition 0.000 claims abstract description 18
- 230000032683 aging Effects 0.000 claims abstract description 14
- 239000011365 complex material Substances 0.000 claims abstract description 13
- 239000000654 additive Substances 0.000 claims abstract description 11
- 230000000996 additive effect Effects 0.000 claims abstract description 11
- 230000007062 hydrolysis Effects 0.000 claims abstract description 11
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 11
- 238000000352 supercritical drying Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003377 acid catalyst Substances 0.000 claims abstract description 9
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims description 23
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- 239000008119 colloidal silica Substances 0.000 claims description 6
- 239000003517 fume Substances 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 238000007598 dipping method Methods 0.000 claims description 5
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 5
- 239000004408 titanium dioxide Substances 0.000 claims description 5
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000003365 glass fiber Substances 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 229920002748 Basalt fiber Polymers 0.000 claims description 3
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 3
- 241000790917 Dioxys <bee> Species 0.000 claims description 3
- 235000007164 Oryza sativa Nutrition 0.000 claims description 3
- 229910003978 SiClx Inorganic materials 0.000 claims description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 239000004917 carbon fiber Substances 0.000 claims description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 229920000728 polyester Polymers 0.000 claims description 3
- 235000009566 rice Nutrition 0.000 claims description 3
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 3
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 2
- RSIHJDGMBDPTIM-UHFFFAOYSA-N ethoxy(trimethyl)silane Chemical compound CCO[Si](C)(C)C RSIHJDGMBDPTIM-UHFFFAOYSA-N 0.000 claims description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 240000007594 Oryza sativa Species 0.000 claims 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 239000011863 silicon-based powder Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 17
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000001467 acupuncture Methods 0.000 abstract description 4
- 230000006835 compression Effects 0.000 abstract description 4
- 238000007906 compression Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 12
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 7
- 239000002585 base Substances 0.000 description 6
- 238000004132 cross linking Methods 0.000 description 6
- 239000003292 glue Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- JZQOJFLIJNRDHK-CMDGGOBGSA-N alpha-irone Chemical compound CC1CC=C(C)C(\C=C\C(C)=O)C1(C)C JZQOJFLIJNRDHK-CMDGGOBGSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 239000011858 nanopowder Substances 0.000 description 4
- 229910000859 α-Fe Inorganic materials 0.000 description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- -1 Under part Substances 0.000 description 3
- 229920002521 macromolecule Polymers 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000004745 nonwoven fabric Substances 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 239000004965 Silica aerogel Substances 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 239000004964 aerogel Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000002742 anti-folding effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910000963 austenitic stainless steel Inorganic materials 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000003605 opacifier Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000000718 radiation-protective agent Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical class [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-IGMARMGPSA-N silicon-28 atom Chemical compound [28Si] XUIMIQQOPSSXEZ-IGMARMGPSA-N 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The present invention relates to a kind of aerosil composite insulation material and preparation method thereof, which carries out hydrolysis the following steps are included: ethyl alcohol, acid catalyst, water and organosilicon are mixed, and obtains hydrolyzate；Hydrolyzate and base catalyst are mixed and carry out polycondensation reaction, obtains colloidal sol；Fiber, hydrophilic silicon-dioxide powdery and function additive are mixed, premix is obtained；Precast body is made using acupuncture apparatus in premix；Under vacuum conditions, precast body is immersed in colloidal sol, is stood, seal aging obtains gel complex material；Gel complex material is subjected to supercritical drying, obtains aerosil composite insulation material.The above method can greatly reduce the dosage of organosilicon, reduce production cost, and the preferable heat-insulating property and resistance to compression tensile property that the material prepared has.
Description
Technical field
The present invention relates to heat-insulating material technical field, more particularly to a kind of aerosil composite insulation material and
Preparation method.
Background technique
Aerosil composite insulation material has fire prevention, hydrophobic, high-efficiency insulated, high resistance to compression, high tensile, height because of it
It is anti-folding etc. excellent characteristics be widely used to electric power, petroleum and petrochemical industry high temperature steam pipeline, thick oil gas filling pipeline, municipal administration heating it is buried
The numerous areas such as pipeline, machinery are kept the temperature, high-speed rail Subway Body is kept the temperature, new-energy automobile is heat-insulated.Building heat preservation is as heat preservation energy-saving
The direction that the maximum market in field and aerosil composite insulation material future are given priority to, when preceding because of its market
Price (1.2~1.5 ten thousand/m3) it is 5~10 times of traditional material price, while in view of the composite factors such as transport and construction, making
Overall cost with aerosil composite insulation material is about 3~6 times of Conventional insulation, is only had in building field
The tentative application of small lot.
, there is the following in the main reason for traditional aerosil composite insulation material high production cost: (1) former
Expect at high cost: traditional technology mostly uses greatly organosilicon as silicon source, such as ethyl orthosilicate, by will be organic in alcohol solvent
Silicon carries out the hydrolysis under acid condition and generates orthosilicic acid, polycondensation is then carried out under alkaline condition, in uniform liquid phase item
Under part, silica is generated, silica contained in aerosil composite insulation material is generated by organosilicon.
1000 kilograms of ethyl orthosilicate (silicon 28) is only possible to produce the silica of 280kg, and organosilicon is at high price；2017 it
Before, a square meter 10mm aerogel material is produced, organic silicon source material cost is as high as 30 yuan, cost accounting nearly 50%.(2) chemical industry
Cost of material increases fast: since 2018, international crude petroleum continuous rise, Environmental Protection in China is increasingly strict, and numerous small chemical factories close
It closes, leads to insufficient supply, organosilicon materials price is gone up by 1.1 ten thousand/ton before 2017 to 1.7 ten thousand/ton, and rise 30% makes
Production cost is more high.
The current expensive production cost of aerosil composite insulation material significantly limits it to building field
The paces of extension, so can aerosil composite insulation material inexpensive in production becomes break through the big market of building
The deciding factor of application；The cost of aerosil composite insulation material is lower, and market is bigger using scale.
Summary of the invention
Based on this, it is necessary to it is compound absolutely to provide a kind of inexpensive aerosil that can effectively reduce organosilicon dosage
The preparation method of hot material.
In addition, the application also provides a kind of aerosil composite insulation material.
A kind of preparation method of aerosil composite insulation material, comprising the following steps:
Organosilicon is carried out to the hydrolysis under acid condition in alcohol solvent, obtains hydrolyzate；
The hydrolyzate is subjected to polycondensation reaction under alkaline condition, obtains colloidal sol；
Fiber, hydrophilic silicon-dioxide powdery and function additive that mass ratio is 1:0.01~0.5:0~0.3 are mixed,
Obtain premix；
The premix is squeezed, precast body is made in needle thorn；
Under vacuum conditions, the precast body is immersed in the colloidal sol, is stood, it is compound to obtain gel for seal aging
Material；
The gel complex material is subjected to supercritical drying, obtains aerosil composite insulation material.
The preparation method of above-mentioned aerosil composite insulation material, hydrophilic silicon-dioxide powdery and function are helped
Agent is first scattered in fiber, is made precast body, then by the precast body be immersed in advance as made from organosilicon hydrolyzation polycondensation it is molten
In glue, silica long chain macromolecule knot is generated except polycondensation reaction occurs between the orthosilicic acid monomer in hydrolyzate under alkaline condition
Outside structure, the surface hydroxyl of orthosilicic acid and its part polycondensation product can also be with the hydroxyl on hydrophilic silicon-dioxide powdery surface in alkalinity
Under the conditions of dehydration condensation occurs, the silica and hydrophilic powder for generating orthosilicic acid are real by chemical bond-O-Si-O-
Existing effect crosslinking, forms an integrally-built g., jelly-like gelinite, the dioxy of effectively insulating is obtained after supercritical drying
SiClx aeroge composite insulation material, it is equal compared to the silica in conventional method aerosil composite insulation material
It is obtained by organosilicon, because of the addition of a large amount of cheap hydrophilic silicon-dioxide powderies in the application, makes the use of organosilicon
Amount is only 1/5~1/2 of organosilicon usage amount in conventional method, greatly reduces production cost.
In addition, dispersing hydrophilic silicon-dioxide powdery and function additive in fiber in advance, precast body is made, parent can be made
Water type silicon-dioxide powdery and function additive are evenly dispersed in the fibre, group crosslinking are advantageously implemented, so that reinforcement material is whole
Structural, the further insulation and tension resistance performance of promotion product of body.
Hydrolysis organosilicon carried out in alcohol solvent under acid condition in one of the embodiments,
The step of obtaining hydrolyzate specifically:
It is 1:0.0~0.04:0.01~0.1:0.05~0.15 ethyl alcohol, acid catalyst, water and organosilicon by mass ratio
Mixing carries out hydrolysis, obtains hydrolyzate；
The step of hydrolyzate is carried out polycondensation reaction under alkaline condition, obtains colloidal sol specifically: be by mass ratio
Hydrolyzate and the base catalyst mixing of 1:0.01~0.08 carry out polycondensation reaction, obtain colloidal sol；
It is fine to be selected from alkali-free glass fiber, high silica fiber, basalt fibre, ceramics for the fiber in one of the embodiments,
At least one of dimension, polyester fiber, oxidization fiber fiber and carbon fiber.
The hydrophilic silicon-dioxide powdery is selected from precipitated silica and vapor phase method hard charcoal in one of the embodiments,
It is at least one of black；The aperture of the hydrophilic silicon-dioxide powdery is 2nm~50nm, and partial size is 5 μm~50 μm.
The function additive is selected from nano zirconium oxide powder, nano alumina powder jointed, nanometer in one of the embodiments,
At least one of magnesium oxide powder, nano-titanium dioxide powder and alpha-iron oxide nano-powder.
The organosilicon is selected from ethyl orthosilicate, methyltriethoxysilane, dimethyl two in one of the embodiments,
At least one of Ethoxysilane and trimethylethoxysilane；The acid catalyst be concentration be 0.1mol/L~
The nitric acid solution or concentration of 0.5mol/L is the sulfuric acid solution of 0.05mol/L~0.25mol/L；The base catalyst is that concentration is
The life of the ammonia spirit of 0.1mol/L~0.5mol/L, the sodium hydroxide solution that concentration is 0.1mol/L~0.5mol/L or saturation
Lime aqueous solution.
The time of the dipping is 20 minutes or more in one of the embodiments, and the time of standing is 1 hour or more,
The time of seal aging is 12 hours or more.
The condition of the vacuum is -0.01MPa or less in one of the embodiments,.
Silica gas made from the preparation method of aerosil composite insulation material described in any of the above embodiments
Gel composite insulation material.
The aerosil composite insulation material is that aerosil is compound in one of the embodiments,
Felt insulation.
Specific embodiment
To facilitate the understanding of the present invention, below will to invention is more fully described, and give it is of the invention compared with
Good embodiment.But the invention can be realized in many different forms, however it is not limited to embodiment described herein.Phase
Instead, purpose of providing these embodiments is makes the disclosure of the present invention more thorough and comprehensive.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein "and/or" includes one or more phases
Any and all combinations of the listed item of pass.
The preparation method of the aerosil composite insulation material of one embodiment, comprising the following steps:
S110, organosilicon is carried out in alcohol solvent to hydrolysis under acid condition, obtains hydrolyzate.
Specifically, step S110 are as follows: by mass ratio be 1:0.01~0.04:0.01~0.1:0.05~0.15 ethyl alcohol,
Acid catalyst, water and organosilicon mixing carry out hydrolysis, obtain hydrolyzate.
Further, for the stability of product, the addition sequence of each raw material in step S110 are as follows: ethyl alcohol, acid catalyst,
Water and organosilicon sequentially add.
Further, acid catalyst is the nitric acid solution or 0.05mol/L~0.25mol/L of 0.1mol/L~0.5mol/L
Sulfuric acid solution.
It is appreciated that by the concentration of the usage ratio and acid that rationally control ethyl alcohol, acid catalyst, water and organosilicon, it can
The pH value of effective control system is in a certain range.
Further, organosilicon is selected from ethyl orthosilicate, methyltriethoxysilane, dimethyl diethoxysilane and three
At least one of methylethoxy base silane.
Further, ethyl alcohol is the food grade ethyl alcohol of 98% or more mass content, in case introducing halide ion, influences product
Use on austenitic stainless steel.
Organosilicon is carried out to the hydrolysis under acid condition in alcohol solvent, obtains orthosilicic acid.
S120, hydrolyzate is subjected to polycondensation reaction under alkaline condition, obtains colloidal sol.
Specifically, step S120 are as follows: mix hydrolyzate and base catalyst that mass ratio is 1:0.01~0.08 and contract
Poly- reaction, obtains colloidal sol.
In the present embodiment, base catalyst be the ammonia spirit of 0.1mol/L~0.5mol/L, 0.1mol/L~
The sodium hydroxide solution of 0.5mol/L or the lime water solution of saturation.
Hydrolyzate is subjected to polycondensation reaction under alkaline condition, polycondensation reaction occurs under alkaline condition between orthosilicic acid monomer
Generate silica long chain macromolecule structure.
S130, by mass ratio be 1:0.01~0.5:0~0.3 fiber, hydrophilic silicon-dioxide powdery and function additive
Mixing, obtains premix.
Wherein, fiber is selected from alkali-free glass fiber, high silica fiber, basalt fibre, ceramic fibre, polyester fiber, oxidization fiber
At least one of fiber and carbon fiber.
In the present embodiment, the diameter of fiber is 3 μm~20 μm, and length is 0.5cm~8cm.
It is appreciated that facilitating hydrophilic silicon-dioxide powdery and function by the diameter and length that rationally control fiber
Auxiliary agent is evenly distributed in the fibre.
Further, hydrophilic silicon-dioxide powdery in precipitated silica and fume colloidal silica at least one
Kind.
Further, the aperture of hydrophilic silicon oxides powder is 2nm~50nm, and partial size is 5 μm~50 μm.
Hydrophilic silicon-dioxide powdery can use SiO2·nH2O indicates, wherein nH2O exists in the form of surface hydroxyl, therefore
Hydrophilic silicon-dioxide powdery is pre-dispersed in after precast body is made in fiber, is immersed in made of organosilicon hydrolyzation polycondensation
In colloidal sol, can the surface hydroxyl under the catalysis of colloidal sol neutral and alkali catalyst with orthosilicic acid and its part polycondensation product be dehydrated
Condensation reaction, so that the silica and hydrophilic silicon-dioxide powdery that generate orthosilicic acid are realized by chemical bond-O-Si-O-
Effectively crosslinking forms an integrally-built g., jelly-like gelinite, can be prepared by the titanium dioxide of effectively insulating through supercritical drying
Silica aerogel composite insulation material effectively reduces the usage amount of organosilicon, reduces and be produced into compared to traditional preparation methods
This, and improve the heat-insulating property and resistance to compression tensile property of product.
Further, function additive is selected from nano zirconium oxide powder, nano alumina powder jointed, nanometer magnesia powder, receives
Rice at least one of titanium dioxide powder and alpha-iron oxide nano-powder.
Wherein, nano zirconium oxide powder, nano alumina powder jointed, nanometer magnesia powder are high temperature resistant filler material；Nanometer
Titanium dioxide powder is high temperature antiradiation agent；Alpha-iron oxide nano-powder is high temperature resistant opacifier.
It should be noted that the sequence of step S130 is unlimited, can before step S110~S120, later carry out,
It can be carried out simultaneously with step S110~S120.
By adjusting fiber, hydrophilic silicon-dioxide powdery and function additive mass ratio be 1:0.01~0.5:0~
0.3, while can making product that there is different function, keep preferable resistance to compression tensile property.
S140, precast body is made through extruding, needle thorn in above-mentioned premix.
Specifically, precast body is made using non-woven fabrics acupuncture apparatus or airlaid acupuncture apparatus in step S140.
Further, precast body is cylindric coiled material, convenient for the uniformity for operating and impregnating.
It is appreciated that precast body is made through extruding, needle thorn in premix, it can make to form uniform gap in precast body, have
Conducive to the infiltration of subsequent colloidal sol, it is advantageously implemented group crosslinking, to keep material overall structure stronger, is further promoted final
The insulation and tension resistance performance of product.
S150, under vacuum conditions, above-mentioned precast body is immersed in colloidal sol, is stood, and it is compound to obtain gel for seal aging
Material.
Wherein, vacuum condition is -0.01MPa or less.
Specifically, in the present embodiment, above-mentioned precast body is fitted into vacuum tank, be evacuated to -0.01MPa with
Under, do not had precast body highest point to be impregnated using negative pressure of vacuum sucking colloidal sol to liquid level.
Further, the time of dipping is 20 minutes or more.The time of standing is 1 hour or more.The time of seal aging
It is 12 hours or more.
In the present embodiment, the time of dipping is 20~30 minutes.The time of standing is 1~3 hour.Seal aging
Time is 12~48 hours.
Stand and the effect of seal aging be: make hydrophilic silicon dioxide nano powder, function additive surface hydroxyl with
And hydrolyzate has time enough to continue that polycondensation reaction occurs, and forms new-O-Si-O- group, stand and seal aging when
Between it is longer, group cross-linking effect is better, and material structure globality is stronger.
S160, above-mentioned gel complex material is subjected to supercritical drying, obtains aerosil composite insulation material.
Specifically, in the present embodiment, above-mentioned premix is set using non-woven fabrics acupuncture apparatus or airlaid needle thorn
The standby volume felt for being woven into preset thickness, rewinding are packed into corresponding coil diameter ruler at the regular cylindrical shape coiled material of the specific coil diameter of fixed width
In very little treating tank；Treating tank lifting is entered in vacuum impregnation tank, -0.01MPa is evacuated to, is sucked using negative pressure of vacuum molten
Glue to liquid level did not had coiled material highest point to be impregnated, and stood, and seal aging obtains gel complex material；By the gel composite wood
Material carries out supercritical drying, obtains aerosil composite adiabatic felt.
The preparation method of above-mentioned aerosil composite insulation material, hydrophilic silicon-dioxide powdery and function are helped
Agent is first scattered in fiber, is made precast body, then by the precast body be immersed in advance as made from organosilicon hydrolyzation polycondensation it is molten
In glue, silica long chain macromolecule knot is generated except polycondensation reaction occurs between the orthosilicic acid monomer in hydrolyzate under alkaline condition
Outside structure, the surface hydroxyl of orthosilicic acid and its part polycondensation product can also be with the hydroxyl on hydrophilic silicon-dioxide powdery surface in alkalinity
Under the conditions of dehydration condensation occurs, the silica and hydrophilic powder for generating orthosilicic acid are real by chemical bond-O-Si-O-
Existing effect crosslinking, forms an integrally-built g., jelly-like gelinite, the dioxy of effectively insulating is obtained after supercritical drying
SiClx aeroge composite insulation material, it is equal compared to the silica in conventional method aerosil composite insulation material
It is obtained by organosilicon, the middle addition because of a large amount of cheap hydrophilic silicon-dioxide powderies, makes making for organosilicon in the application
Dosage is only 1/5~1/2 of organosilicon usage amount in conventional method, greatly reduces production cost.
The following are specific embodiments.
Embodiment 1
It is that the ethyl alcohol of 1:0.01:0.01:0.05, the nitric acid solution of 0.2mol/L, water and ethyl orthosilicate mix by mass ratio
Reaction is hydrolyzed in conjunction, obtains hydrolyzate；
The ammonia spirit of hydrolyzate and 0.3mol/L that mass ratio is 1:0.01 is mixed and carries out polycondensation reaction, is obtained molten
Glue；
By mass ratio be the alkali-free glass fiber of 1:0.01:0.15:0.15, (aperture 5nm, partial size are 6 μ to precipitated silica
M), nano zirconium oxide powder and nano alumina powder jointed mixing, obtain premix；
Precast body is made through extruding, needle thorn in premix, precast body is fitted into vacuum tank, be evacuated to-
0.01MPa did not had precast body highest point to be impregnated using negative pressure of vacuum sucking colloidal sol to liquid level, and control dip time is 20 points
Clock stands 1 hour, seal aging 12 hours, obtains gel complex material；
Gel complex material is subjected to supercritical drying, obtains aerosil composite insulation material.
Embodiment 2
It is the ethyl alcohol of 1:0.04:0.1:0.15, the sulfuric acid solution of 0.25mol/L, water and methyl triethoxy by mass ratio
Reaction is hydrolyzed in silane mixture, obtains hydrolyzate；
The sodium hydroxide solution of hydrolyzate and 0.5mol/L that mass ratio is 1:0.08 is mixed and carries out polycondensation reaction, is obtained
Colloidal sol；
By mass ratio be 1:0.5:0.1:0.1 ceramic fibre, fume colloidal silica (aperture 20nm, 20 μm of partial size), receive
Rice titanium dioxide powder and alpha-iron oxide nano-powder mixing, obtain premix；
Precast body is made through extruding, needle thorn in premix, precast body is fitted into vacuum tank, be evacuated to-
0.01MPa did not had precast body highest point to be impregnated using negative pressure of vacuum sucking colloidal sol to liquid level, and control dip time is 30 points
Clock stands 3 hours, seal aging 48 hours, obtains gel complex material；
Gel complex material is subjected to supercritical drying, obtains aerosil composite insulation material.
Embodiment 3
It is the ethyl alcohol of 1:0.02:0.05:0.10, the sulfuric acid solution of 0.05mol/L, water and dimethyl diethoxy by mass ratio
Base silane mixing carries out hydrolysis, obtains hydrolyzate；
The lime water solution of hydrolyzate and saturation that mass ratio is 1:0.04 is mixed and carries out polycondensation reaction, is obtained molten
Glue；
By ceramic fibre and fume colloidal silica (aperture 50nm, partial size are 50 μm) mixing that mass ratio is 1:0.3, obtain
To premix；
Precast body is made through extruding, needle thorn in premix, precast body is fitted into vacuum tank, be evacuated to-
0.01MPa did not had precast body highest point to be impregnated using negative pressure of vacuum sucking colloidal sol to liquid level, and control dip time is 25 points
Clock stands 2 hours, seal aging 24 hours, obtains gel complex material；
Gel complex material is subjected to supercritical drying, obtains aerosil composite insulation material.
Comparative example 1
Comparative example 1 is substantially the same manner as Example 3, unlike, after fume colloidal silica is mixed with colloidal sol in comparative example 1
It is used further to the fiber preform that dipping is only prepared by ceramic fibre.
Comparative example 2
Comparative example 2 is substantially the same manner as Example 3, unlike, the matter of ceramic fibre and fume colloidal silica in comparative example 2
Amount is than being 1:1.
The performance of aerosil composite insulation material prepared by Examples 1 to 3 and comparative example 1~2 is shown in Table 1.
Table 1
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of preparation method of aerosil composite insulation material, which comprises the following steps:
Organosilicon is carried out to the hydrolysis under acid condition in alcohol solvent, obtains hydrolyzate；
The hydrolyzate is subjected to polycondensation reaction under alkaline condition, obtains colloidal sol；
Fiber, hydrophilic silicon-dioxide powdery and function additive that mass ratio is 1:0.01~0.5:0~0.3 are mixed, obtained
Premix；
The premix is squeezed, precast body is made in needle thorn；
Under vacuum conditions, the precast body is immersed in the colloidal sol, is stood, seal aging obtains gel complex material；
The gel complex material is subjected to supercritical drying, obtains aerosil composite insulation material.
2. the preparation method of aerosil composite insulation material according to claim 1, which is characterized in that described
The step of organosilicon is carried out to the hydrolysis under acid condition in alcohol solvent, obtains hydrolyzate specifically:
It is that 1:0.01~0.04:0.01~0.1:0.05~0.15 ethyl alcohol, acid catalyst, water and organosilicon mix by mass ratio
Reaction is hydrolyzed, obtains hydrolyzate；
The step of hydrolyzate is carried out polycondensation reaction under alkaline condition, obtains colloidal sol specifically: by mass ratio be 1:
0.01~0.08 hydrolyzate and base catalyst mixing carries out polycondensation reaction, obtains colloidal sol.
3. the preparation method of aerosil composite insulation material according to claim 1, which is characterized in that described
Fiber is in alkali-free glass fiber, high silica fiber, basalt fibre, ceramic fibre, polyester fiber, oxidization fiber fiber and carbon fiber
At least one.
4. the preparation method of aerosil composite insulation material according to claim 1, which is characterized in that described
Hydrophilic silicon-dioxide powdery is selected from least one of precipitated silica and fume colloidal silica；The hydrophilic titanium dioxide
The aperture of silicon powder is 2nm~50nm, and partial size is 5 μm~50 μm.
5. the preparation method of aerosil composite insulation material according to claim 1, which is characterized in that described
Function additive is selected from nano zirconium oxide powder, nano alumina powder jointed, nanometer magnesia powder, nano-titanium dioxide powder and receives
At least one of rice ferric oxide powder.
6. the preparation method of aerosil composite insulation material according to claim 1, which is characterized in that described
Organosilicon is in ethyl orthosilicate, methyltriethoxysilane, dimethyl diethoxysilane and trimethylethoxysilane
At least one；The nitric acid solution or 0.05mol/L~0.25mol/L that the acid catalyst is 0.1mol/L~0.5mol/L
Sulfuric acid solution；The base catalyst is the hydrogen-oxygen of the ammonia spirit of 0.1mol/L~0.5mol/L, 0.1mol/L~0.5mol/L
Change the lime water solution of sodium solution or saturation.
7. the preparation method of described in any item aerosil composite insulation materials according to claim 1~6, feature
It is, the time of the dipping is 20 minutes or more, and the time of standing is 1 hour or more, and the time of seal aging is 12 hours
More than.
8. the preparation method of described in any item aerosil composite insulation materials according to claim 1~6, feature
It is, the vacuum condition is -0.01Mpa or less.
9. dioxy made from the preparation method of aerosil composite insulation material according to any one of claims 1 to 8
SiClx aeroge composite insulation material.
10. aerosil composite insulation material according to claim 9, which is characterized in that the silica
Aeroge composite insulation material is aerosil composite adiabatic felt.
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